An analytical method has been developed for the separation and determination of naturally occurring radionuclides (primordial and its decay products in ore samples and liquid wastes from mining and milling process. The radionuclides include U-238, Th-232, Ra-226, Pb-210 and Po-210. The methodology involves three steps: 1. Complete sample dissolution by wet oxidation. 2. Sequential separation of radionuclides by ion exchange and co-precipitation. 3. Radiometric determination by alpha, beta and gamma counting spectroscopy. The detection limit for a radiochemical yield of approximately 72%, was 0.28 mBq per sample for Th-232, U-238 and Po-210. To test it's applicability, the method was used with standard ore samples, soil and sediment. The analytical procedure was applied to a large number of liquid waste samples and the results of these analysis are presented.
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